IS 1528 (Part 13) :2007 1S0 12676:2000 Indian Standard METHODS OF SAMPLING AND PHYSICAL TESTS FOR REFRACTORY MATERIALS PART 13 DETERMINATION ( OF RESISTANCE TO CARBON MONOXIDE Second Revision) ICS 81.080 @ BIS 2007 BUREAU MANAK September2007 OF INDIAN STANDARDS ZAFAR MARG BHAVAN, 9 BAHADUR SHAH NEW DELHI 110002 Price Group 3 Refractories Sectional Committee, MTD 15 NATIONAL FOREWORD This Indian Standard (Part 13) (Second Revision) which is identical with 1S0 12676:2000 `Refractory products -- Determination of resistance to carbon monoxide' issued by the International Organization for Standardization (ISO) was adopted by the Bureau of Indian Standards on the recommendation of the Refractories Sectional Committee and approval of the Metallurgical Engineering Division Council. This standard was originally published in 1962 and subsequently revised in 1974. This revision of the standard has been taken up to align it with ISO 12676 : 2000 by adoption, under dual numbering system. The text of ISO Standard has been approved as suitable for publication as an Indian Standard without deviations. Certain conventions are, however, not identical to those used in Indian Standards. Attention is particularly drawn to the following: a) Wherever the words `International Standard' appear referring to this standard, they should be read as `Indian Standard'. b) Comma (,) has been used as a decimal marker, while in Indian Standards, practice is to use a point (.) as the decimal marker. the current In this adopted standard, reference appears to the following International Standard for which Indian Standard also exists. The corresponding Indian Standard, which is to be substituted in its place, is listed below along with its degree of equivalence for the edition indicated: International Standard Corresponding Indian Standard Degree of Equivalence ISO 5022 : 1979 products testing -- Sampling Shaped refractory and acceptance IS 1528 (Part 7) : 1974 Methods of sampling and physical tests for refractory materials: Part 7 Methods of sampling and criteria for conformity (first revision) Technically Equivalent The technical committee responsible for the preparation of this standard has reviewed the provision of the following International Standard and has decided that it is acceptable for use in conjunction with this standard: International Standard Title ISO 8656-1:1988 Refractory products -- Sampling of raw materials and unshaped -- Part 1: Sampling scheme products For the purpose of deciding whether a particular requirement of final value, observed or calculated, expressing the result of a test accordance with IS 2 : 1960 `Rules for rounding off numerical significant places retained in the rounded off value should be the in this standard. this standard is complied with, the or analysis, shall be rounded off in The number of values (revised)'. same as that of the specified value IS 1528 (Part 13):2007 ISO 12676:2000 Indian Standard METHODS OF SAMPLING AND PHYSICAL TESTS FOR REFRACTORY MATERIALS PART 13 DETERMINATION (Second 1 Scope Standard specifies a method for determining disintegration. the comparative resistance of refractory materials to OF RESISTANCE TO CARBON MONOXIDE Revision ) This International carbon monoxide The test is intended to be more severe than conditions encountered of refractory materials to be assessed in a relatively short time. in service in order to enable probable behaviour 2 Normative references The following normative documents contain provisions which, through reference in this text, constitute provisions of this International Standard. For dated references, subsequent amendments to, or revisions of, any of these publications do not apply. However, parties to agreements based on this International Standard are encouraged to investigate the possibility of applying the most recent editions of the normative documents indicated below. For undated references, the latest edition of the normative document referred to applies. Members of ISO and IEC maintain registers of currently valid International Standards. ISO 5022:1979, ISO 8656-1:1988, scheme. Shaped refractory Refractory products -- Sampling and acceptance testing. products -- Part 1: Sampling products -- Sampling of raw materials and unshaped 3 Terms and definitions For the purposes of this International 3.1 Standard, the following terms and definitions apply. carbon monoxide disintegration breakdown of a refractory product caused by the deposition of carbon resulting from the dissociation of carbon monoxide 3.2 carbon monoxide resistance resistance of a refractory product to carbon monoxide disintegration ified conditions of atmosphere and temperature when exposed to carbon monoxide under spec- 4 Principle at a controlled temperature when carrying Test pieces are exposed to a specified carbon monoxide atmosphere NOTE Carbon the atmosphere for a specified time monoxide is toxic and suitable safety precautions should be observed around the apparatus to detect leakage of carbon monoxide. out this test e.g. monitoring 1 IS 1528( Part13) ISO 12676:2000 :2007 5 Apparatus examples of test apparatus Schematic are shown in Figure 1 2\ 8 4 /' /3 ------+ 5 Key 1 2 3 4 5 6 7 8 9 Furnace enclosure Gas exit tube Reaction Gas-tight chamber end cap Test piece support Test pieces Gas inlet tube Temperature Tube support measuring device Figure 1 -- Examples of test apparatus (schematic: not to scale) 2 IS 1528( Part13) ISO 12676:2000 :2007 5.1 Furnace, ofsufficient * 10 `C at 500 "C. sizetobe capable ofmaintaining thetest zonewithin thereaction chamber (5.2) towithin NOTE The furnace may be fitted with one or more observation ports to enable direct observation of the test samples during the test when a glass reaction chamber is used. 5.2 Reaction chamber, comprising a gas-tight tube capable of withstanding a temperature of 500 "C and made of a material which does not react with carbon monoxide under the conditions of the test. The chamber shall be of a suitable size to accommodate the test pieces (see clause 7) within the test zone. It shall be fitted with gas inlet and outlet tubes so that the gas passes through the length of the test zone. Provision shall be made for the insertion of a temperature measuring and recording device (5.3) to be located in the test zone and adjacent to the test pieces. The chamber shall also contain supports on which to rest the test pieces and to prevent debris from falling into the chamber in cases of disintegration during the test. The tubes and the support shall also be of a material unreactive to carbon monoxide and capable of withstanding temperatures of up to 500 "C. NOTE 1 Suitable materials for the reactionchamberare certain grades of stainless steel, brass, aluminium, unoxidisedinconel metal, glass and ceramic. NOTE 2 The reaction chamber maybe closed at one end and one of the gas tubes used together with a second tube to carry the test piece support so long as the criteria above are maintained. Depending on the size of the reaction chamber and the number of test pieces, it may be necessary to provide support for the tubes themselves. 5.3 Temperature measuring and recording device, to enable the temperature the required accuracy (see 5.1 ) and to be continuously recorded. 5.4 5.5 of the test zone to be measured to Temperature controller, to control the furnace (5.1) to the required accuracy. Carbon monoxide, of 99 O/.purity. NOTE 1 The carbon monoxide maybe supplied from gas bottles or a tank depending on the size of the reaction chamber and the gas flow required (see 8.6). If large quantities of CO are required then it may be purified to the above specification and recirculated, NOTE 2 When carbon monoxide inlet tube [see 5.7 b)]. is supplied from a tank, iron carbonyl may be present in the gas and may cause clogging of the 5.6 5.7 a) Nitrogen, of industrial grade. Means of control of carbon monoxide atmosphere, operating as follows: for gas supplied by tank or bottle, the pressure shall be reduced by a regulator made for that purpose and the flow of gas adjusted by means of a sensitive needle or regulating valve. a purification train shall be situated after the fine control valve and consist of a drying tower (silica gel, magnesium perchlorate or phosphorus pentoxide may be used but not sulphuric acid or calcium chloride). If the gas is supplied from a tank follow the drying tower with a scrubbing tower to remove iron carbonyl (e.g. containing sodium hydroxide pellets). the gas flow rate shall be measured using a suitable non-aqueous and jhe reaction chamber inlet tube. flowmeter fitted between the purification train b) c) 5.8 Reaction chamber pressure control, a bubbling bottle or sensitive pressure gauge shall be fitted to the outlet of the reaction chamber to ensure that a positive pressure, of at least 20 mm of water, is maintained throughout the test. 5.9 Gas analyser, capable of determining a maximum of 5 0/0 carbon dioxide. 5.10 the carbon dioxide content of the exhaust gas to ensure that it contains Drying oven, capable Desiccator. of maintaining a temperature of 110 `C + 5 "C. 5.11 3 IS 1528 (Part 13):2007 ISO 12676:2000 5.12 5.13 Timer Photographic equipment. 6 Sampling products or The number of items to be tested shall be determined in accordance with ISO 5022 for shaped products or a sampling plan agreed between the interested parties. ISO 8656-1 for unshaped 7 Test pieces 7.1 General Test pieces shall be rectangular prisms with a 50 mm * 2 mm, 64 mm & 2 mm or 76 mm * 2 mm square crosssection. The length of the prisms shall be agreed between the interested parties but shall be a minimum of 76 mm. NOTE 1 It is recommended that only test pieces from one material are included in each test to avoid the behaviour of one mate- rial affecting NOTE 2 the behaviour of another. Care should be taken when cutting the test pieces from larger test items that the cut surfaces are not contaminated with alloy which may originate from iron or iron-containing the type of cutting equipment used. 7.2 Fired materials Only one test piece shall be taken from each test item and cut so that a minimum of three faces are the original surfaces of the test item. 7.3 Unfired materials Test pieces of unfired materials shall be prepared according to the manufacturers' instructions or in an appropriate manner according to the type of material. Alternatively, test pieces may be cut from larger prepared shapes. The test pieces shall be fired in an oxidizing atmosphere at a rate not exceeding 5 OC/min to a temperature 540 "C, maintained at this temperature for 5 h, then cooled and stored in the desiccator (5.11). of NOTE 1 Cylindrical test pieces of unfired materials cut before or after firing to 540 `C may be used. The test pieces shall be of a diameter of 50 mm * 2 mm and a minimum length of 76 mm. NOTE 2 In cases where large numbers of samples require testing or for quality control purposes, made on the basis of test results using small test pieces (e.g. 30 mm x 30 mm x 30 mm). non-referee evaluations maybe 8 8.1 8.2 Procedure Dry test pieces of fired materials at 110 `C+ 5 "C and allow to cool in the desiccator (5.1 1). Place the cooled test pieces on the supports in the test zone of the reaction chamber so that they are separated by at least 20 mm in order to allow free circulation of gas. 8.3 Insert the temperature chamber. measuring device (5.3) and ensure it is located properly (see 5.2). Seal the reaction 8.4 Thoroughly flush ;he chamber with nitrogen (5.6) and heat the test pieces to 500 `C + 10 `C whilst continuing to pass nitrogen through the chamber. 4 IS 1528 (Part 13):2007 ISO 12676:2000 8.5 When the test pieces have attained the test temperature, cease the nitrogen flow and change the atmosphere to a minimum of 95 O/. in order carbon monoxide (5.5) as shown by analysis of the exhaust gas. Record the time and date. NOTE This may be done by flushing the nitrogen with a high flow of carbon monoxide or by evacuating the chamber with a vacuum pump to a pressure of about 100 mmHg (1 mmHg = 133,3224 Pa), then introducing carbon monoxide at a flow rate indicated in 8.6. The process is then repeated until the required exhaust gas analysis is obtained. 8.6 Regulate the flow of carbon monoxide (5.5) to a nominal rate of not less than 30 cm3ih for each 15 cm3 of total specimen volume. Analyse the exhaust gas after 1 h and if it is less than 95 0/0 carbon monoxide, increase the gas flow. Repeat the analysis and flow rate adjustment until the exhaust gas is above957. carbon monoxide. Analyse the exhaust gas at least twice a day during the duration of the test and maintain the chamber atmosphere above 95 % carbon monoxide. NOTE The initial flow rate of 30 cm3/h for each 15 cm3 of total specimen volume is considered to be a minimum rate with which to carry out the test. For materials suspected of reacting significantly with carbon monoxide, a flow rate 2 to 3 times greater may be required to maintain the chamber atmosphere. In these cases, it may be advisable to reduce size and number of test pieces m the chamber in order to avoid excessive use of carbon monoxide. 8.7 Continue the test for 200 h, at which time change to a flow of nitrogen to flush out the furnace chamber. Switch off the furnace and allow the chamber to cool. Record time and date at which the test was terminated, carefully remove the test pieces, inspect their condition in accordance with clause 9 and make a photographic record of their appearance. NOTE corded. 1 If the test apparatus has facilities for direct observation of the test pieces, then daily inspections can be made and re- The test can then be terminated when the test piece or half the number of test pieces show disintegration (see clause 9). that the NOTE 2 A shorter or longer test duration may be agreed between interested parties. It must, however, be recognised clauses describing the test piece condition [see 9 a) 1) to 4)] will only be comparable for the same test duration. 9 a) Condition The condition 1) 2) unaffected: surface of test pieces of the test pieces no carbon shall be described surface or spalis according to the following observable; classifications: deposition, pop-outs pop-outs or cracking damage. surface 10 mm or less in diameter visible; 3) cracked. cracks visible within the test pieces, and/or spans or surface pop-outs greater than 10 mm in diameter have occurred; disruphon: test pieces have broken into two or more pieces, or when hand pressure can cause breaking. of the test pieces is variable, the number of test pieces in each classification shall be stated. 4) b) If the condition 10 Test report information: The test report shall include the following a) b) c) d) e) f) g) h) the name of the test establishment; the time and date at which the test was commenced reference to this International any deviations designation Standard, and terminated; i.e. ISO 12676; in the test procedure; type, brand, etc.); of material tested (manufacture, the number of items tested; the size of the test pieces; the duration of the test; IS 1528 (Part 13):2007 ISO 12676:2000 1) the flow rate (expressed tion; the cond!tlon in cm3/h per cm~ of total test piece volume) used during the major part of the test dura- J) k) of the test pieces; In relation according to the classiflcahons or the performance of the results; if necessary, in clause 9; those made during the test, any observa,!;on If any, which to the test pieces of the test, including may assist record in the interpretation of the test pieces, 1) the photographic 6 Bureau of Indian Standards of /rrdian marking Standards Act, 1986 to promote and quality certification of goods BIS is a statutory institution established under the Bureau harmonious development of the activities of standardization, and attending to connected matters in the country. Copyright No part of these publications may be reproduced in any BIS has the copyright of all its publications. form without the prior permission in writing of BIS. This does not preclude the free use, in course of implementing the standard, of necessary details, such as symbols and sizes, type or grade designations. Enquiries relating to copyright be addressed to the Director (Publications), BIS. Review of Indian Standards Amendments are issued to standards as the need arises on the basis of comments. Standards are also reviewed periodically; a standard along with amendments is reaffirmed when such review indicates that no changes are needed; if the review indicates that changes are needed, it is taken up for revision. Users of Indian Standards should ascertain that they are in possession of the latest amendments or edition by referring to the latest issue of `BIS Catalogue' and `Standards: Monthly Additions'. This Indian Standard has been developed from Dot: No. MTD 15 (4706). 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